CN115337454B

CN115337454B - Device and method for preparing composite modified film layer of nano structure on surface of dental implant

Info

Publication number: CN115337454B
Application number: CN202210976402.XA
Authority: CN
Inventors: 肖桂勇; 王银川; 陈歆; 吕宇鹏
Original assignee: Shandong University
Current assignee: Shandong University
Priority date: 2022-08-15
Filing date: 2022-08-15
Publication date: 2023-04-18
Anticipated expiration: 2042-08-15
Also published as: CN115337454A

Abstract

The invention belongs to the technical field of biomedical engineering, and provides a device and a method for preparing a composite modified film layer of a nano structure on the surface of a dental implant, wherein a plurality of dental implant fixing ports are fixed on the edge of a rotary disc, and the rotary disc can be driven to rotate by a first power mechanism, so that titanium-based dental implants on the dental implant fixing ports at different positions of the rotary disc sequentially enter an alkali liquor storage device for alkali heat treatment; the titanium-based dental implant subjected to the alkali heat treatment is conveyed to one end of a horizontal moving device under the driving of a first power mechanism, and meanwhile, an induction heating coil is moved to the titanium-based dental implant position by the horizontal moving device to perform induction heating treatment on the titanium-based dental implant; through the arrangement of the first power mechanism, the horizontal moving device, the rotary table and the like, the alkali heat and induction heating of the titanium-based dental implant can be quickly realized, the automation degree and the working efficiency are high, and the automatic heating device is suitable for mass production.

Description

Preparation device and method of composite modified film layer with nano structure on surface of dental implant

Technical Field

The invention belongs to the technical field of biomedical engineering, and particularly relates to a device and a method for preparing a composite modified film layer of a nano structure on the surface of a dental implant.

Background

Because of low density, excellent mechanical property and good biocompatibility, titanium metal is widely applied to the field of dental implant clinical medicine. However, the titanium metal has poor bone induction capability and is rendered biologically inert, and the integration mode with bone tissues is mainly physical integration, so that effective chemical bonding is lacked, and the treatment effect is finally influenced. Therefore, the titanium-based dental implant needs to be surface modified to improve the bioactivity and osteoinductivity by changing the surface composition, morphology, roughness and the like. At present, most of titanium-based dental implants used clinically adopt a surface treatment process of sand blasting and acid etching, and although the preparation process can improve the biological activity of the titanium-based dental implant, the biological activity of the titanium-based dental implant needs to be further improved.

The inventors have found that alkaline heat treatment and surface oxidation are common methods for surface modification of titanium metals. The alkali heat treatment can enable a layer of porous sodium titanate gel active layer to be generated on the surface of the titanium metal, and the existence of the sodium titanate gel layer can effectively induce the deposition of hydroxyapatite on the surface of the titanium metal, so that the bonding capability between the dental implant and the bone is enhanced. However, the abrasion resistance of the gel layer needs to be further improved. The surface oxidation method can prepare titanium dioxide (rutile and anatase) oxide films on the surfaces of titanium metal, can effectively improve the wear resistance of the titanium metal, and can well promote the deposition of hydroxyapatite on the surfaces of the titanium metal. The induction heating oxidation is a green and environment-friendly rapid oxidation technology, and can quickly form a layer of uniformly-grown titanium dioxide oxide film on the surface of titanium metal, so that the biological activity and the wear resistance of the titanium dioxide oxide film are effectively improved. However, the alkali heat treatment and the induction heating oxidation need to be carried out step by step, the preparation process is complex, and the preparation efficiency in a laboratory is low. Therefore, how to automatically and efficiently prepare the nano-structure composite modified film layer on the surface of the titanium-based dental implant is realized has important significance for further improving the clinical application value and realizing commercial production.

Disclosure of Invention

The invention aims to solve the problems, provides a device and a method for preparing a nano-structure composite modified film layer on the surface of a dental implant, can quickly realize automatic alkali heat and induction heating of a titanium-based dental implant, forms a porous composite modified film layer rich in sodium titanate and titanium dioxide on the surface of the titanium-based dental implant, has simple preparation process and high automation degree and working efficiency, and is suitable for mass production.

In order to achieve the above object, in a first aspect, the present invention provides a device for preparing a composite modified film layer with a nano structure on the surface of a dental implant, which adopts the following technical scheme:

a tooth planting body surface nano structure composite modification rete preparation facilities includes:

the output end of the first power mechanism is provided with a rotary disc; a plurality of dental implant fixing openings are fixed at the edge of the side surface of the rotary disc, which is far away from the first power mechanism;

the alkali liquor storage device is arranged at the lower end of the rotary disc, one part of the rotary disc is positioned in the alkali liquor storage device, and the other part of the rotary disc is positioned outside the alkali liquor storage device;

and the horizontal moving device is arranged at the upper end of the turntable, and one end of the horizontal moving device, which is close to the turntable, is provided with an induction heating coil.

Further, a heating sleeve is arranged outside the alkali liquor storage device; the upper end of the alkali liquor storage device is provided with a liquor injection port, and the lower end of the alkali liquor storage device is provided with a liquor outlet.

Further, the first power mechanism is a motor, and a first gear is mounted on the output shaft; a connecting rod is vertically fixed in the middle of the rotary table, and a second gear meshed with the first gear is fixed at one end, far away from the rotary table, of the connecting rod.

Furthermore, a plurality of dental implant fixing openings are uniformly distributed on the circumferential direction of the rotating disc.

Furthermore, the horizontal moving device comprises a moving cross rod and a vertical rod, and an induction heating coil is fixed at one end of the vertical rod, which is far away from the moving cross rod; the movable cross rod is connected with a second power mechanism.

Further, the second power mechanism is a motor, and a third gear is fixed on an output shaft of the motor; and a rack meshed with the third gear is arranged on the movable cross rod.

Further, both ends of the movable cross rod are provided with racks, and both ends of the movable cross rod are provided with second power mechanisms.

Further, the device further comprises a controller, and the controller is connected with the first power mechanism and the second power mechanism.

In order to achieve the above object, in a second aspect, the present invention further provides a method for preparing a composite modified film layer with a nanostructure on the surface of a dental implant, which adopts the following technical scheme:

a method for preparing a nano-structured composite modified film on the surface of a dental implant, which adopts the apparatus for preparing a nano-structured composite modified film on the surface of a dental implant according to any one of claims 1 to 8, comprising:

securing a plurality of untreated titanium-based dental implants to a dental implant fixture; adding alkali liquor into an alkali liquor storage device through a liquor injection port;

controlling a first power mechanism to immerse the titanium-based dental implant in alkali liquor for alkali heat treatment;

controlling a first power mechanism to enable the titanium-based dental implant subjected to alkali heat treatment to be positioned at the position which is at the same horizontal line with the induction heating coil;

controlling a second power mechanism to enable the titanium-based dental implant to be positioned in the center of the induction heating coil; and induction heating the titanium-based dental implant.

Further, the alkali liquor is sodium hydroxide solution; the concentration of the alkali liquor is 4-12mol/L, the alkali heating time is 10-30h, and the alkali heating temperature is 40-80 ℃; the induction heating frequency is 10-100kHz, the induction heating power is 10-50kW, and the induction heating time is 10-40s.

Compared with the prior art, the invention has the beneficial effects that:

1. according to the invention, a plurality of dental implant fixing openings are fixed on the edge of a rotary disc, and the rotary disc can be driven to rotate by a first power mechanism, so that titanium-based dental implants on the dental implant fixing openings at different positions of the rotary disc sequentially enter an alkali liquor storage device for alkali heat treatment; the titanium-based dental implant subjected to the alkali heat treatment is conveyed to one end of a horizontal moving device under the driving of a first power mechanism, and meanwhile, an induction heating coil is moved to a titanium-based dental implant implantation position by the horizontal moving device to perform induction heating treatment on the titanium-based dental implant; through the arrangement of the first power mechanism, the horizontal moving device, the rotary table and the like, the alkali heat and induction heating of the titanium-based dental implant can be quickly and automatically realized, and a porous composite modified film rich in sodium titanate and titanium dioxide is formed on the surface of the titanium-based dental implant, so that the preparation process is simple, the automation degree and the working efficiency are high, and the preparation method is suitable for mass production;

2. the automatic system for preparing the nano-structure composite modified film by performing alkaline heating and induction heating on the titanium-based dental implant, which is designed by the invention, has the advantages of simple preparation process, high working efficiency, environmental friendliness and suitability for mass production.

3. Compared with the titanium-based dental implant used clinically at present, the porous nano-structured sodium titanate and titanium dioxide-rich composite film prepared on the surface of the titanium-based dental implant has more excellent bioactivity.

Drawings

The accompanying drawings, which form a part hereof, are included to provide a further understanding of the present embodiments, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the present embodiments and together with the description serve to explain the embodiments and are not intended to limit the embodiments to the proper form disclosed herein.

FIG. 1 is a schematic structural view of example 1 of the present invention;

FIG. 2 is an XRD pattern of the surface of a titanium-based dental implant prepared according to example 1 of the present invention;

FIG. 3 is an SEM photograph of the surface of a titanium-based dental implant prepared according to example 1 of the present invention;

wherein, 1, an alkali liquor storage device; 11. a liquid injection port; 12. a liquid outlet; 13. alkali liquor; 2. a turntable; 21. a dental implant fixation port; 22. a connecting rod; 23. a first gear; 3. a titanium-based dental implant; 4. a first power mechanism; 41. a first motor output shaft; 42. a second gear; 5. a horizontal moving device; 51. moving the cross bar; 52. a vertical rod; 53. a second power mechanism; 54. a second motor output shaft; 55. a third gear; 56. a rack; 6. an induction heating coil; 7. and a controller.

Detailed Description

The invention is further described with reference to the following figures and examples.

It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.

Example 1:

as shown in fig. 1, the present embodiment provides a device for preparing a composite modified film with a nanostructure on a dental implant surface, which includes an alkali solution storage device 1, a solution injection port 11, a solution outlet 12, an alkali solution 13, a rotary table 2, a dental implant fixing port 21, a connecting rod 22, a first gear 23, a titanium-based dental implant 3, a first power mechanism 4, a first motor output shaft 41, a second gear 42, a horizontal moving device 5, a moving cross rod 51, a vertical rod 52, a second power mechanism 53, a second motor output shaft 54, a third gear 55, a rack 56, an induction heating coil 6, and a controller 7;

the output end of the first power mechanism 4 is provided with the turntable 2; a plurality of dental implant fixing openings 21 are fixed at the edge of the side surface of the rotary disc 2 far away from the first power mechanism 4; the dental implant fixing port 21 is used for fixing a titanium-based dental implant, and the size of the dental implant fixing port 21 is matched with that of the bottom of the titanium-based dental implant; a plurality of dental implant fixing ports 21 are uniformly distributed in the circumferential direction of the rotary table 2;

the alkali liquor storage device 1 is arranged at the lower end of the rotary table 2, one part of the rotary table 2 is positioned in the alkali liquor storage device 1, and the other part of the rotary table 2 is positioned outside the alkali liquor storage device 1;

the horizontal moving device 5 is arranged at the upper end of the turntable 2, and an induction heating coil 21 is arranged at one end, close to the turntable 2, of the horizontal moving device 5.

Specifically, a platform and a frame may be provided, the lye storage device 1 is disposed on the platform, and the first power mechanism 4, the second power mechanism 53 and the controller are fixed at corresponding positions by means of bolts or welding.

A heating jacket is arranged outside the lye storage device 1, the arrangement of the heating jacket belongs to the conventional arrangement, and details are not described herein, for example, a jacket-shaped structure with heating elements such as heating wires is arranged outside the lye storage device 1; the upper end of the alkali liquor storage device 1 is provided with a liquor injection port 11, and the lower end is provided with a liquor outlet 12; it is understood that the liquid filling port 12 may be provided with a detachable plug. The heating jacket outside the lye storage device 1 can also be provided with a temperature control device.

The first power mechanism 4 is a first motor, and a second gear 42 is mounted on an output shaft 41 of the first motor; a connecting rod 22 is vertically fixed at the middle position of the rotary disc 2, and a first gear 23 meshed with the second gear 42 is fixed at one end of the connecting rod 22 far away from the rotary disc 2. Specifically, the connecting rod 22 may be rotatably disposed on the frame through a bearing and the like, so that the connecting rod 22 is fixed to the frame in the axial direction, and when the second gear 42 drives the first gear 23 to rotate, the connecting rod 22 may be driven to rotate, so as to rotate the turntable 2.

The horizontal moving device 5 comprises a moving cross rod 51 and a vertical rod 52, and an induction heating coil 6 is fixed at one end of the vertical rod 52 far away from the moving cross rod 51; the movable cross rod 51 is connected with a second power mechanism 53; specifically, the second power mechanism 53 may be a second motor, and a third gear 55 is fixed on the output shaft 54 of the second motor; the movable cross bar 51 is provided with a rack 56 meshed with the third gear 55; it can be understood that the movable cross bar 51 can be connected with the frame through a slide rail and a slide groove, etc. matching mechanisms, so as to realize the horizontal movement function. The diameter of the induction heating coil 6 can be matched with that of the titanium-based dental implant 3 so as to realize uniform heating of the bottom and the top of the thread of the titanium-based dental implant 3.

Racks 56 are arranged at two ends of the movable cross rod 51, and second power mechanisms 53 are arranged at two ends of the movable cross rod 51; the two second power mechanisms 53 simultaneously drive the movable cross bar 51 to ensure the stability thereof.

The controller 7 may be connected to the first power mechanism 4 and the second power mechanism 53 to drive the first power mechanism 4 and the second power mechanism 53.

The main working process or principle of the embodiment is as follows:

s1, fixing a plurality of untreated titanium-based dental implants 3 on a dental implant fixing port 21; adding alkali liquor 13 into the alkali liquor storage device 1 through the liquor injection port 11;

s2, controlling a first motor to immerse the titanium-based dental implant 3 in an alkali liquor 13 for alkali heat treatment;

s3, controlling a first motor to enable the titanium-based dental implant subjected to alkali heat treatment to be positioned at the position which is the same horizontal line with the induction heating coil 6;

s4, controlling a second motor to enable the titanium-based dental implant to be positioned in the center of the induction heating coil 6; and carrying out induction heating on the titanium-based dental implant.

Specifically, the alkali solution 13 in step S1 may be a sodium hydroxide solution or a potassium hydroxide solution; sodium hydroxide solution can be selected, and the sodium hydroxide is lower in cost and easy to obtain. In the step S2, the concentration of the alkali liquor 13 is 4-12mol/L, the alkali heating time is 10-30h, and the alkali heating temperature is 40-80 ℃. S4, controlling the induction heating frequency to be 1-30MHz, the induction heating power to be 5-50kW and the induction heating time to be 5-50S; it can be set that the induction heating frequency is 10-100kHz, the induction heating power is 10-50kW, and the induction heating time is 10-40s.

Example 2:

the embodiment provides a method for preparing a composite modified film with a nano structure on the surface of a dental implant, which adopts a device for preparing the composite modified film with the nano structure on the surface of the dental implant as described in the embodiment 1, and comprises the following steps:

The alkali liquor is sodium hydroxide solution; the concentration of the alkali liquor is 4-12mol/L, the alkali heating time is 10-30h, and the alkali heating temperature is 40-80 ℃; the induction heating frequency is 10-100kHz, the induction heating power is 10-50kW, and the induction heating time is 10-40s.

Specifically, S1, fixing a titanium-based dental implant 13 on a titanium-based dental implant fixing port;

s2, injecting 10mol/L sodium hydroxide solution into the alkali liquor storage device 1, and controlling the temperature of the alkali liquor to be constant at 60 ℃ by using an electric heating sleeve;

s3, controlling a first motor, rotating the turntable 2, and immersing the titanium-based dental implant 3 in a sodium hydroxide solution for alkaline washing for 12 hours;

s4, controlling a first motor, rotating a turntable, and positioning the titanium-based dental implant obtained by the processing in the step S3 at the position which is the same horizontal line with the center of the induction heating coil 6;

s5, controlling a second motor, moving the induction heating coil 6 to the position of the turntable, enabling the titanium-based dental implant to be located at the center of the inside of the induction heating coil 6, and starting induction heating, wherein the rated power is 50kW, the frequency is 25kHz, and the time is 10S;

and S6, controlling a second motor, moving the induction heating coil to a position far away from the turntable, unloading the titanium-based dental implant obtained in the step S5, and fixing the untreated titanium-based dental implant again. And (4) repeating the steps S3-S6 to rapidly prepare a large amount of titanium-based dental implants with porous surfaces and rich in sodium titanate and titanium dioxide oxide films.

As can be seen from FIG. 2, the prepared titanium-based dental implant surface contains sodium titanate, anatase and rutile phases in addition to the matrix titanium. As can be seen from FIG. 3, the titanium-based dental implant surface has a sponge-like porous structure with an average pore diameter of about 200 nm.

In other embodiments, the sodium hydroxide concentration used may be set at 5mol/L, and the alkaline heat time may be set at 24h; the induction heating power may be set to 45kW, the induction heating frequency may be set to 20kHz, and the induction heating time may be set to 20s.

The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and those skilled in the art can make various modifications and variations. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present embodiment should be included in the protection scope of the present embodiment.

Claims

1. The utility model provides a compound modified rete preparation facilities of dental implant surface nano-structure which characterized in that includes:

the output end of the first power mechanism is provided with a turntable; a plurality of dental implant fixing openings are fixed at the edge of the side surface of the rotary disc, which is far away from the first power mechanism;

the alkali liquor storage device is arranged at the lower end of the rotary disc, one part of the rotary disc is positioned in the alkali liquor storage device, and the other part of the rotary disc is positioned outside the alkali liquor storage device; a heating sleeve is arranged outside the alkali liquor storage device;

the horizontal moving device is arranged at the upper end of the turntable, and one end of the horizontal moving device close to the turntable is provided with an induction heating coil; by controlling the first power mechanism, the titanium-based dental implant can be immersed in alkali liquor for alkali heat treatment; by controlling the first power mechanism, the titanium-based dental implant subjected to alkali heat treatment can be positioned at the same horizontal line position with the induction heating coil.

2. The apparatus for preparing a nano-structured composite modified film on the surface of a dental implant according to claim 1, wherein the alkaline solution storage device is provided with a solution inlet at the upper end and a solution outlet at the lower end.

3. The apparatus for preparing a nano-structured composite modified film on the surface of a dental implant according to claim 1, wherein the first power mechanism is a motor, and a second gear is mounted on an output shaft of the motor; a connecting rod is vertically fixed in the middle of the turntable, and a first gear meshed with the second gear is fixed at one end of the connecting rod, which is far away from the turntable.

4. The apparatus for preparing a nano-structured composite modified film on the surface of a dental implant according to claim 1, wherein a plurality of dental implant fixing ports are uniformly distributed in the circumferential direction of the rotary disk.

5. The device for preparing the nano-structured composite modified film on the surface of the dental implant according to claim 1, wherein the horizontal moving device comprises a moving cross bar and a vertical bar, and an induction heating coil is fixed at one end of the vertical bar, which is far away from the moving cross bar; the movable cross rod is connected with a second power mechanism.

6. The apparatus for preparing a nano-structured composite modified film on the surface of a dental implant according to claim 5, wherein the second power mechanism is a motor, and a third gear is fixed on an output shaft of the motor; and a rack meshed with the third gear is arranged on the movable cross rod.

7. The apparatus for preparing a nano-structured composite modified film on the surface of a dental implant according to claim 6, wherein the movable cross bar is provided with racks at both ends thereof, and the movable cross bar is provided with second power mechanisms at both ends thereof.

8. The apparatus for preparing a composite modified film with a nanostructure on the surface of a dental implant according to claim 7, further comprising a controller, wherein the controller is connected to the first power mechanism and the second power mechanism.

9. A method for preparing a nano-structured composite modified film on the surface of a dental implant, which is characterized in that the device for preparing the nano-structured composite modified film on the surface of the dental implant according to any one of claims 1 to 8 is used, and comprises the following steps:

10. The method for preparing the nano-structured composite modified film on the surface of the dental implant according to claim 9, wherein the alkaline solution is a sodium hydroxide solution; the concentration of the alkali liquor is 4-12mol/L, the alkali heating time is 10-30h, and the alkali heating temperature is 40-80 ℃; the induction heating frequency is 10-100kHz, the induction heating power is 10-50kW, and the induction heating time is 10-40s.